Black cotton dye.



UNITED STATES PATENT OFFICE.

CHRISTOPHER RIS, OF BASLE, SWITZERLAND, ASSIGNOR TO JOHN R.

' GEIGY & 00., OF SAME PLACE.

BLACK COTTON DY E.

SPECIFICATION forming part of Letters Patent No. 636,066, dated. October 31, 1899.

Application filed J'i'lne 3, 1899. Serial N0- 7l9,282. (Specimena) To all whom it may concern:

Be it known that I, CHRISTOPHER RIs, a citizen of the Republic of Switzerland, residingin Basle, in the Republic of Switzerland, have invented certain new and useful Black Cotton Dyes, of which the following is aspecification.

The present invention refers to new black coloring-matters especially useful for dyeing cotton fast=black shades, said coloring-matters being obtained by melting a paraamidophenol compoundsuch as paraamidophenol paraamidocresol (CH OH NH 1:2 5)With acetyl compounds and sulfur at a temperature from about 200 to 300 centigrade. To the melting mixture a diluent may be added in order to accomplish a moderate reactionas, for instance, glycerin, ethyleneglycol, chlorhydrin, kresol, anthracene, naphtalene, and analogous substances.

Example I: Forty-four kilos of paraamidophenol, twen ty-six kilos of acetanilid, and forty kilos of sulfur are melted together in a vessel furnished with a stirring mechanism at a temperature of 210 to 230 centigrade till the development of sulfureted hydrogen will almost be finished. Then the mass is pulverized. In order to dissolve the same, it isboiled with about five hundred liters of water and fifty kilos of caustic-soda lye of 40 Baum, after which the solution is precipitated by addition of acids or of bicarbonate of sodium and the coloring-matter filtered off, pressed, dried, and pulverized. It forms a black powder difficultly soluble in hot water with dark greenish-blue color, soluble in diluted caustic-alkali lye with dark bluish-black color, easily soluble in a watery solution of sodium sulfid with olive color, difi'icultly soluble in alcohol with greenish-blue color, insoluble in ether and benzene, soluble in concentrated sulfuric acid with bluish-black color. When dissolved in a solution of sodium sulfid and evaporated to dryness, it forms a black powder easily soluble in water with olive color, insoluble in alcohol, ether, and benzene, and soluble in concentrated sulfuric acid with olive-black color.

Example II: Sixty kilos of the coloring matter of Example I are dissolved in about five hundred liters of boiling water, with addition of ninety kilos of crystallized sodiumsulfid. Then the solution is evaporated to siccity, best in a vacuum, and the coloringmatter pulverized. In a hot bath containing sodium sulfid and common salt or Glaubers salt th e color dyes unmordanted cotton dark blackish-olive shades, which turns, by means of oxidizing agentssuch as oxygen of the air, bichromate of potasse, sulfate of copper, or chlorid of ironinto deep black of great fastness.

Example III: Forty four kilos of paraamidophenol, thirty kilos of paraamidoacet anilid, thirty kilos of glycerin, and forty kilos of sulfur are meltedas described in the first example and also further treated in the same manner. The thus-obtained coloring-matter shows almost the same properties as that of the first example. Its solution in concentrated sulfuric acid is of a dark greenish-black. It dyes unmordanted cotton in a hot bath of sodium sulfid and salt dark olive-black shades, which turn by oxidation into deep black.

In these examples instead of the named acetyl compounds other acetyl compounds may be used, such as acetoluidins, acetxylidins, acetnaphtylamids, paraoxyacetanilid, paranitroacetanilid, paraamidoacetorthotoluidin. The thus-formed coloring-matters show the same properties as above described. The respective quantities of amidophenols, acetyl compounds, sulfur, and diluent may be varied, as also the temperature from 200 to about 300 oentigrade.

The chemical constitution of the new 001- ors cannot yet be ascertained.

I claim- As an article of manufacture, the new black dyestufi obtained from paraamidophenol, an acetyl compound and sulfur, which forms a black powder easily soluble in Water with an olive color, soluble in concentrated sulfuric acid with olive-black color, insoluble in alcohol, ether and benzene, and possessing the dyeing properties substantially as described.

In testimony that I claim theforegoing as my invention I have signed my name in pres ence of two subscribing witnesses.

CHRISTOPHER RIS.

Witnesses:

GEORGE GIFFoRD, JOHN G. PLATNER. 

